Aluminum(III) Chloride → 5-Fluoro-1-indanone

HRID 375598

반응식

HRID 375598 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[CH2:5][CH2:6][C:7](Cl)=[O:8].[Cl-].[Al+3].[Cl-].[Cl-]>C(=S)=S>[F:1][C:2]1[CH:3]=[C:4]2[C:10](=[CH:11][CH:12]=1)[C:7](=[O:8])[CH2:6][CH2:5]2

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 189935013-(3-Fluorophenyl)propanoyl chloride

생성물 1

HCID 1365375-Fluoro-1-indanone수율 16.1%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매2회

실험 절차

A solution of 3-fluorodihydrocinnamoyl chloride (15.4 g) in carbon disulfide (78 ml) was added dropwise to a cold (-5° C.) mixture of aluminium chloride (13.9 g) in carbon disulfide (300 ml) for 30 minutes. During this time and for 30 minutes the mixture was allowed to warm to room temperature (1 hr), then it was heated to reflux (1 hr) and finally the volatiles were removed by distillation under reduced pressure. The residue was dissolved in methylene chloride (400 ml) and washed successively with 10% aqueous sodium hydroxide and water. After drying (magnesium sulfate) and solvent removal in vacuo, 5-fluoroindanone (2 g) was isolated by recrystallisation from hexane.

후처리

  1. temperatureit was heated
  2. temperatureto reflux (1 hr)
  3. customfinally the volatiles were removed by distillation under reduced pressure
  4. dissolutionThe residue was dissolved in methylene chloride (400 ml)
  5. washwashed successively with 10% aqueous sodium hydroxide and water
  6. customAfter drying
  7. custom(magnesium sulfate) and solvent removal in vacuo

출처 및 근거

ORD 기록
ord-e4074e4510fa425b95af15b30757d78f
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05486541

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